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Method for preparing high-purity trimethyl antimony from trimethyl aluminum and antimony trichloride

A technology of trimethyl antimony and trimethyl aluminum, applied in the direction of antimony organic compounds, etc., can solve the problems of long time, difficult trimethyl antimony, dangerous to handle, etc., and achieves high safety, simple operation and high purity. Effect

Active Publication Date: 2021-11-02
安徽亚格盛电子新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] At present, there is little research on the preparation process of trimethyl antimony at home and abroad. Its normal pressure boiling point is 80.6 ° C and is similar to that of most solvents and impurities, which makes it very difficult to obtain high-purity trimethyl antimony. Now the recognized synthesis method It uses ether as a solvent to prepare the Grignard reagent methylmagnesium iodide and then reacts with antimony trichloride to synthesize trimethyl antimony crude product. After complicated post-processing, it is not only time-consuming and very dangerous to handle, but also impurity water and solvents are difficult to obtain. In addition to cleaning to affect its purity

Method used

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  • Method for preparing high-purity trimethyl antimony from trimethyl aluminum and antimony trichloride

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example 1

[0021] This embodiment provides a method for preparing high-purity trimethylantimony by using trimethylaluminum and antimony trichloride, the steps are as follows:

[0022] Step 1: Take 456.5g or 2.0mol of antimony trichloride, first heat it at 45°C and dry it in vacuum under absolute pressure, add the above antimony trichloride into a 2L four-necked bottle in an anhydrous and oxygen-free environment, and set up a normal pressure reflux device , keep the airtightness good, and start stirring;

[0023] Step 2: Set the cold oil in the condenser tube to -10±1°C, pass through the cold oil, and slowly add 432.5g or 6.0mol of trimethylaluminum dropwise when the temperature of the cold oil drops to the set temperature. Aluminum from slow to fast, after the addition of trimethylaluminum, adjust the temperature to 95°C and stir for 5 hours;

[0024] Step 3: Slowly increase the temperature of the reaction bottle, the maximum temperature is controlled at 120°C, and the temperature at th...

example 2

[0029] This embodiment provides a method for preparing high-purity trimethylantimony by using trimethylaluminum and antimony trichloride, the steps are as follows:

[0030] Step 1: Take 684.5g, that is, 3.0mol of antimony trichloride, and first heat it to 45°C for absolute pressure vacuum drying, add the above antimony trichloride into a 2L four-necked bottle in an anhydrous and oxygen-free environment, set up an atmospheric distillation device, and gas Good tightness, start stirring;

[0031] Step 2: Set the cold oil in the condenser tube to -10±1°C, pass through the cold oil, and slowly add 648.5g or 9.0mol of trimethylaluminum dropwise when the temperature of the cold oil drops to the set temperature. Aluminum from slow to fast, after the trimethylaluminum is added dropwise, the temperature is raised to 96°C and the reaction is stirred for 5 hours;

[0032] Step 3: Slowly increase the temperature of the reaction bottle, the maximum temperature is controlled at 120°C, and t...

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Abstract

The invention aims to provide a method for preparing high-purity trimethyl antimony from trimethyl aluminum and antimony trichloride, which comprises the following steps: trimethyl aluminum is reacted with antimony trichloride to generate trimethyl antimony and dimethyl aluminum chloride; the by-product methylaluminum chloride reacts with metal sodium under the condition of a catalyst sodium fluoride to generate trimethylaluminum, the trimethylaluminum continues to react with antimony trichloride to generate trimethyl antimony, the safety is high, the synthesis yield of trimethyl antimony is high, the purity is high, other organic impurities are not easy to introduce, and the operation is simple.

Description

technical field [0001] The invention relates to the field of metal-organic source synthesis, in particular to a method for preparing high-purity trimethylantimony by using trimethylaluminum and antimony trichloride. Background technique [0002] In recent years, the application of semiconductors has become more and more widespread, and has broad application prospects in semiconductor lighting, new generation mobile communications, smart grids, high-speed rail transit, new energy vehicles, consumer electronics and other fields. Semiconductor materials are supporting information, energy, transportation, Key new materials for the development of national defense and other industries. Metal-organic chemical vapor deposition (MOCVD) technology is an advanced and effective method for manufacturing compound semiconductor ultra-thin film materials, and high-purity metal-organic compounds (MO source) are the supporting source materials for the modern compound semiconductor industry. ...

Claims

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Application Information

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IPC IPC(8): C07F9/90
CPCC07F9/90
Inventor 姜永要许澄城张俊杰
Owner 安徽亚格盛电子新材料有限公司
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